Molecular structure of silsesquioxanes determined by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry
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Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry was used to deduce the three-dimensional structure of a complex silsesquioxane polymer. Four distinct levels of structure were observed in the mass spectrum. The overall shape of the peak distribution was typical of polymers formed by condensation reactions. The mass separation between major clusters of peaks, each major cluster corresponding to an oligomer with a unique number of repeat units, confirmed that the synthesis proceeded as expected with no side reactions. The mass separation between peaks within a major cluster showed that intramolecular reactions during synthesis resulted in the elimination of water. The loss of water was ascribed to the formation of closed loops in the polymer structure. A simple arithmetic algorithm is presented for identifying these peaks. Autocorrelation techniques were used to determine the number and distribution of intramolecular closed loops per oligomer. This knowledge was used to deduce whether a particular oligomer is branched-linear, ladder, polyhedral, or some combination of these. The single-oligomer isotopic distribution was used to determine that cationization was present from both sodium and potassium ions.
- Baney, R. H.; Itoh, M.; Sakakibara, A.; Suzuki, T. Chem. Rev. 1995, 95, 1409–1430. CrossRef
- Voronkov, M. G.; Lavrent’yev, V. I. In Inorganic Ring Systems Boschke, F. L., Ed.; Springer: Berlin, 1982; pp 199–236.
- Lichtenhan, J. D.; Vu, N. Q.; Carter, J. A.; Gilman, J. W.; Feher, F. J. Macromolecules 1993, 26, 2141–2142. CrossRef
- Lichtenhan, J. D.; Otonari, Y. A.; Carr, M. J. Macromolecules 1995, 28, 8435–8437. CrossRef
- Sellinger, A.; Laine, R. M. Macromolecules 1996, 29, 2327–2330. CrossRef
- Zhang, C.; Laine, R. M. J. Organomet. Chem. 1996, 521, 199–201. CrossRef
- Sellinger, A.; Laine, R. M. Chem. Mater. 1996, 8, 1592–1593. CrossRef
- Haddad, T. S.; Lichtenhan, J. D. Macromolecules 1996, 29, 7302–7304. CrossRef
- Crivello, J. V.; Malik, R. J. Polym. Sci.: Part A: Polym. Chem. 1997, 35, 407–425. CrossRef
- Antonucci, J. M.; Fowler, B. O.; Stansbury, J. W. ACS Polym. Preprints 1997, 38, 118–119.
- Pan, Q.; Gonzalez, G. B.; Composto, R. J.; Wallace, W. E.; Arkles, B.; Figge, L. K.; Berry, D. H., Thin Solid Films, in press.
- Gentle, T. E. In Rapid Thermal and Integrated Processing Moslehi, M. M.; Singh, R.; Kwong, D. L., Ed.; SPIE: Bellingham, WA, 1991; pp 146–164.
- Hacker, N. P. MRS Bull 1997, 22(10), 33–38.
- Mantz, R. A.; Jones, P. F.; Chaffee, K. P.; Lichtenhan, J. D.; Gilman, J. W.; Ismail, I. M. K.; Burmeister, M. J. Chem. Mater. 1996, 8, 1250–1259. CrossRef
- Gilman, J. W.; Kashiwagi, T.; Harris, R. H.; Lomakin, S.; Lichtenhan, J. D.; Bolf, A.; Jones, P. Proc. Additives98 Conf., in press.
- Agaskar, P. A.; Klemperer, W. G. Inorg. Chim. Acta 1995, 229, 355–364. CrossRef
- Belu, A. M.; DeSimone, J. M.; Linton, R. W.; Lange, G. W.; Friedman, G. W. J. Am. Soc. Mass Spectrom. 1996, 7, 11–24. CrossRef
- Hensel, R. R.; King, R. C.; Owens, K. G. Rapid Commun. Mass Spectrom. 1997, 11, 1785–1793. CrossRef
- Certain commercial equipment is identified in this article in order to specify adequately the experimental procedure. In no case does such identification imply recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the items identified are necessarily the best available for the purpose.
- McEwen, C. N.; Jackson, C.; Larsen, B. S. Int. J. Mass Spectrom. Ion Processes 1997, 160, 387–394. CrossRef
- Birdi, K. S. Fractals in Chemistry, Geochemistry, and Biophysics: An Introduction; Plenum: New York, 1993, Chap 8.
- Owens, K. G. Appl. Spectrosc. Rev. 1992, 27, 1–49. CrossRef
- Molecular structure of silsesquioxanes determined by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry
Journal of the American Society for Mass Spectrometry
Volume 10, Issue 3 , pp 224-230
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